Extractor assembly

ABSTRACT

APPARATUS AS A NEW AND IMPROVED EXTRACTOR ASSEMBLY FOR CONSECUTIVE HOT SOLVENT EXTRACTION, VAPOR AND VAPOR CONDENSATE EXTRACTION.

'5. L. RANDALL BXTRACTOR ASSEMBLY March 19, 1974 3 Sheets-Sheet 1 Filed Oct.

FIG. 3

PIC-3.4

FIG. 2

March 19, 1974 E. L RANDALL 3,798,133

EXTRACTOR ASSEMBLY Filed Oct. 18, 1971 3 Sheets-Sheet 2 FIG- 5 FIG. 6

March 19, 1974 E- L. RANDALL EXTRACTOR ASSEMBLY 3 Sheets-Sheet 3 Filed Oct. 18, 1971 3,798,133 EXTRACTOR ASSEMBLY Edward L. Randall, 8615 Erinbrook Way, Sacramento, Calif. 95826 Filed Oct. 18, 1971, Ser. No. 190,064 Int. Cl. B01d 11/02 US. Cl. 203-99 9 Claims ABSTRACT OF THE DISCLOSURE Apparatus as a new and improved extractor assembly for consecutive hot solvent extraction, vapor and vapor condensate extraction.

This invention relates to an improved extraction apparatus assembly and, moreparticularly, to the new and improved extractor assembly for obtaining consecutive hot solvent extraction followed by vapor and vapor condensate extraction.

Existing equipment for solvent extraction for quantitative analysis require that the extraction take place either entirely as a hot solvent extraction or entirely as a vapor condensate extraction. It is recognized that an improved extractor which allows hot solvent and vapor and vapor condensate extraction of a sample is desirable. Especially if easily adaptable to fat analysis of meat and meat products as well as fat analysis of grain and stock feeds.

Apparatus which permits rapid and accurate extraction is highly desirable.

It must be appreciated that existing apparatus as described requires extensive periods of extraction. It is common to require up to 6 hours for a normal hot solvent extraction. As described in (AOAC, 10th edition, 1965), Crude Fat or Ether Extract, Direct Method- Official, Final Action, Determination at page 331, 1122.033, indicates that the extraction period may vary from 4 hours at condensation rate of -6 drops per second to 16 hours at 2-3 drops per second.

Objects of the present invention are to provide for an improved extractor assembly to improve the efliciency of extraction, such that less time is needed for the completion of the desired extraction. In general, to improve construction and operation of solvent-vapor extractors.

Another object is to provide an improved process for consecutive extraction of extractable material.

Other objects and features of the invention will be more apparent from the following description when considered with the following drawings in which:

FIG. 1 is a side elevation of a longitudinal movable slidable suspension means 8 and means for holding a sample container 18.

FIG. 2 is a perspective view of a sample container assembly.

FIG. 3 is a sectional view showing a substantially vertical double flow condenser, representative of a condensing means for condensing solvent vapors.

FIG. 4 is a perspective view of a container means for a solvent.

FIG. 5 is a section taken through an assembled extractor, taken on a plane parallel to the longitudinal movable slidable suspension means 8 with a sample container assembly in place.

FIG. 6 is an enlarged detail section of the solvent container with the sample container assembly in an elevated position on a plane parallel to a longitudinal movable slidable suspension means.

FIG. 7 is an assembled view of the extractor assembly with a cut-away section showing the respective relationships of the various parts.

In the following description and in the claims, various details will be identified by specific names for conven- United States Patent 0 3,798,133 Patented Mar. 19, 1974 ience but they are intended to be as generic in their application as the art will permit.

Like reference characters denote like parts in the several figures of the drawings.

In the accompanying drawings and description forming part of this specification, certain specific disclosure of the invention is made for purposes of explanation, but it will be understood that the details may be modified in various respects without departure from the broad aspect of the invention.

Referring now to the accompanying drawings and more particularly to FIGS. 5 and 6 which are a schematic elevation of laboratory apparatus suitable as an improved solvent and vapor extractor. For a more specific embodiment of this invention, reference is also made to FIGS. 1, 2, 3 and 4.

As illustrated, the improved extractor comprises a solvent containing means 5 which is adapted to communicate with an eflicient condensing means 1, such as a dual flow condenser. The main body of the condenser 1 preferably includes a lower portion 4 which is adapted to communicate with the solvent container 5. Shown in the drawings is a condenser adapted to communicate by an annular opening at its lower portion with a complementary annular opening on the solvent containing means. The annular opening at the lower portion of the condensing means is provided with sealing means for sealing against vapor leakage when in communication with the complementary annular opening on the solvent containing means. Said sealing means may be accomplished in any number of a variety of Ways, for example, as shown in the drawings, planar ground glass connections on each annular opening held securely in communication by a detachable clamping means 6. Other sealing means contemplated herein include, pairs of complementary tapered ground glass joints, complementary ball joint fittings, O- ring sealing joints and the like. The condensing means 1 and solvent containing means 5 are firmly held in place during the extraction process by a suitable detachable clamping means 6. After the extraction is complete, the detachable clamping means 6 allows detachment of the solvent container 5 to permit completion of the desired analysis.

Said condensing means 1 is provided with an internal lower guide means 3 for directing the placement of the detachable movable longitudinal slidable suspension means 8. Said movable slidable suspension means 8 is adapted at its lower portion with mounting means 18 for detachably mounting a sample container assembly 7 and 9.

As shown in FIG. 2 the sample container assembly is represented as comprising two components: A porous thimble 7 constructed of porous material which allows rapid passage of the solvent to permeate the sample within the thimble and to pass with the dissolved material into the solvent container 5. Similarly, when the sample container is in an elevated configuration for the vapor extraction FIG. 6 the porous thimble 7 allows the vapors and condensed vapors to permeate the sample. The condensed vapors return to the solvent container below. The sample container also comprises a screen basket '9. The basket 9 is so constructed of rigid porous screen that the thimble 5 can rest within the basket during the extraction processes both as a hot solvent extraction and as a vapor extraction. The basket 9 is constructed preferably of an inert metal, such as stainless steel, but can also be made from various non-metallic screen-like material, such as various inert plastics.

In conjunction with the slidable suspension means 8 the sample container assembly 7 and 9 is securely but detachably mounted thereto at its lower extremity by the mounting means 18. The means for detachably mounting the sample container assembly may be of various types and in a variety of ways, the only requirement being that the sample container assembly 7 and 9 is detachable from said slidable suspension means and that it is securely held in position once placed within the condenser 1 and solvent container 5. Thus, a pin or pins may be used, slottedgroove arrangement, or as shown in FIGS. 1 and an alternating misaligned series of elongations. The sample container complementary therewith and held by opposing forces.

The internal upper guide means 2 and internal lower guide means 3 are positioned within the main body of the condensing means. The slidable suspension means 8 extends the entire length of the condenser with a portion of the slidable suspension means extending above the open end 11 of the condensing means 1. The slidable suspension means 8 is extended through the internal upper control guide means 2 through the body of the condenser and through the internal lower control guide means 3 and into the adjoined solvent container 5. At the lower portion of the slidable suspension means 8 removably aflixed thereto 18 is a sample container assembly 7 and 9.

Said internal guide means, upper 2 and lower 3, aid in orienting the slidable suspension means 8 Within the condenser and at the same time aid to orient the sample within the central portion of the apparatus. The internal guide means may be constructed of any inert material, such as glass, stainless steel or plastic material. The drawings show the guide means, 2 and 3, are securely and rigidly attached to opposite sides of the condenser body. In the center of said guide means is a slot, hole or other central opening, which allows the slidable suspension means 8 to freely pass therethrough. It is preferred that the central openings within the internal guide means 2 and 3 are aligned substantially with the vertical axis of the condensing means 5.

In a preferred embodiment, a slidable suspension means 8 is slidably mounted within the passageway of the condenser 1 and positioned in the internal guide means 2 and 3 in the condenser. By the portion of the slidable suspension means extending exteriorly above the condenser through the opening 11, one is able to move the slidable suspension means 8 to adjust the positioning of the sample container assembly 7 and 9 so that it is either in the solvent in the solvent container 5 or immediately above the solvent in the vapor space. A stationary selected position can be achieved by various mechanical expedient means for locking the slidable suspension means 8. With this manner of manipulation of a slidable suspension means 8, an operator is able to achieve orientation of the sample container assembly 7 and 9 for hot solvent extraction and vapor condensate extraction without dismantling the apparatus. Where'by the slidable suspension means movably mounted in said condensing means 5, said slidable suspension means upon movement thereof, being operative to vary the effective interaction between said hot solvent in the solvent container 5 and said sample container assembly 7 and 9. It is to be understood that movements of the slidable suspension means may be obtained by any number of mechanically expedient means for varying the effective positioning thereof; and that means for locking said slidable suspension means 8 with attached sample container assembly 7 and 9 at a selected position above the hot solvent within the vapor space therea'bove, but below the condensing means 1 is also provided for within the contemplation of this invention. Said vapor space is formed by the communication of the solvent container 5 and the condensing means described herein.

During the operation of the extractor assembly, a sample which has been accurately weighed into a sample container assembly 7 and 9, is removably affixed to the slidable suspension means 8 at 18 and is lowered into the solvent container 5 as shown in FIG. 5 approximately onethird filled with a suitable solvent. In this configuration,

the apparatus permits hot extraction of the sample in the sample container assembly 7 and 9. With reference to FIG. 6, the slidable suspension means 8 with the attached sample container assembly 7 and 9 at 18 is activated into a raised position, shown in FIG. 6, so that the sample container assembly is positioned above the solvent and below the reflux return. Continued heating of the solvent to reflux now permits a vapor condensate extraction of the sample. The vapor condensate extraction is accomplished as the hot solvent vapors rise up into the condenser 1. As the hot vapors pass the raised sample container assembly 7 and 9, FIG. 6, the porous thimble 7 and basket 9 permit free entry, wetting, bathing and extraction of the sample therein. The solvent condensate then falls into the raised sample container 7 and 9 and provides an extraction and rinsing effect. The solvent condensate then falls into the solvent container 5. The vapors rising from the heated solvent in the solvent container 5 extracts the sample in the sample container assembly 7 and 9 and drains into the remaining solvent below the raised sample container assembly.

By means of the present invention, it is thus possible to subject a sample to hot solvent extraction and vapor and vapor condensate extraction utilizing the same apparatus. It is not necessary to subject a sample to high temperatures for long periods of time. Similarly, it is not necessary to dismantle the apparatus used for a hot solvent extraction and transfer the sample to an apparatus for vapor condensate extraction.

The apparatus and process of this invention can be used conveniently for the extraction of fat from meat or grain and stock feed samples.

It is also to be noted that the solvent container 5 is heated by an appropriate heating means for obtaining the boiling and reflux of the selected solvent.

Broadly considered, the invention is dependent upon the relative positioning of the sample container 7 and 9 within the hot solvent in a solvent containing means 5, FIG. 5, and the positioning of a sample container assembly 7 and 9 above the boiling solvent as it emits solvent vapors, FIG. 6. The sample container must be at some time within the solvent and at some time above the boiling solvent in the vapor space so that the sample container is thoroughly and effectively wetted to saturation.

The primary advantages, therefore, of the present invention are the rapid wetting of the sample and effective extraction thereof; and the elimination of long period of vapor and condensed vapor extraction which is for the most part slow and inefficient. The former advantage is accomplished by positioning the sample container assembly 7 and 9 into the solvent in the solvent containing means 5. The latter advantage is accomplished by so positioning the sample container assembly 7 and 9 by the slidable suspension means 8, such that the sample container assembly is in the hot vapor space immediately above the solvent. By the cooperative interaction of these two steps, it is possible to obtain accurate quantiaive analysis by the extractive processes of hot solvent extraction and vapor and vapor condensate extraction. It is also specifically to be noted that the time required to complete a given extraction is considerably reduced when employing the apparatus and method of this invention.

The assembled apparatus or any part thereof of this invention may be fastened in a variety of ways to suitable support means for positioning and firmly holding in place above a suitable heating means. It is also contemplated within this invention that a locking means for the positioning of the slidable suspension means 8 can be integrated into the support means and adapted to the portion of the slidable suspension means extending exteriorly above the condensing means. As fastening means, there may be employed clamps, bolts, straps, and the like.

While certain novel features of the invention have been disclosed herein, and are pointed out in the annexed claims, it will be understood that, in accordance with the doctrine of equivalents various omissions, substitutions and changes may be made by those skilled in the art without departing from the spirit of the invention.

What is claimed is:

1. An extraction apparatus comprising:

(a) a condensing means for condensing solvent vapors,

said condensing means having an upper annular opening, a lower annular opening with scalable means for communication with a solvent container;

(b) a container means for holding solvent having an annular upper opening complementary to said lower annular opening of said condensing means and sealable therewith;

(c) a longitudinally slidable suspension means for positioning a sample container within said container means, said slidable suspension means having a lower extremity and an upper extremity, from said condensing means said upper extremity extending exteriorly so that said sample container can be longitudinally adjustably positioned in a plane parallel to said longitudinal slidable suspension means;

(d) mounting means aflixed to said lower extremity of said longitudinally slidable suspension means within the condensing means and container means;

(e) a sample container assembly detachably mounted to said longitudinally slidable suspension means at said lower extremity thereof.

2. The apparatus of claim 1 wherein said longitudinally slidable suspension means is provided with adjusting means for locking said longitudinally slidable suspension means with attached mounted sample container at selected positions within said condensing means and solvent containing means.

3. The apparatus of claim 2 wherein said adjusting (a) positioning a sample in a sample container assembly in a solvent in a solvent container, said solvent container communicating with a condensing means and scalable therewith, said sample container assembly detachably mounted to the lower extremity of a slidable suspension means, said slidable suspension means extending an upper extremity exteriorly therefrom;

(b) heating the solvent in said solvent container;

(c) raising and locking said sample container assembly to a position immediately above the heated solvent in the vapor space formed by the communication of the solvent container and condensing means;

(d) heating the solvent in said solvent container to produce solvent vapors, thereby, wetting, bathing and extracting said sample in said sample container assemy;

(e) condensing said solvent vapors in the condensing means and returning the condensate to the solvent container.

7. The method of claim 6, wherein said slidable suspension means extends from the sample container through said condensing means and is available exteriorly for raising and positioning said sample container assembly.

8. The method of claim 6 wherein said sample container assembly is a porous thimble and porous basket container therefor.

9. The apparatus of claim 1 wherein said sample container assembly comprises a porous thimble and po rous basket.

References Cited UNITED STATES PATENTS 1,536,259 5/1925 De Lacy 202 1,562,870 11/1925 Daniels 23272.6 S 1,010,991 12/1911 Walter et a1. 202-169 X 2,732,415 1/1956 Keinge 202-168 X NORMAN YUDKOFF, Primary Examiner D. EDWARDS, Assistant Examiner US. Cl. X.R. 

